P
US9079833B2ActiveUtilityPatentIndex 90

Process for the preparation of a polysulfide

Assignee: KLOBES OLAFPriority: Apr 12, 2011Filed: Apr 10, 2012Granted: Jul 14, 2015
Est. expiryApr 12, 2031(~4.8 yrs left)· nominal 20-yr term from priority
Inventors:KLOBES OLAFHE JING
C07C 319/24C08G 75/14
90
PatentIndex Score
48
Cited by
50
References
11
Claims

Abstract

Process for the preparation of polysulfide of formula (I) HS—(CH 2 ) n —O—(CH 2 ) m —O—(CH 2 ) p —[S—S—CH 2 ) n O—(CH 2 ) m —O—(CH2) p ] q —SH (I) wherein m is an integer in the range 1 to 4, n and p are integers in the range 1-10, and q is an integer in the range 1-60, by oxidizing a bismercaptodiether compound of formula (II) HS—(CH 2 ) n —O—(CH 2 ) m —O—(CH 2 ) p —SH (II) with elemental sulfur in the presence of a base and a protic solvent. This process has a high selectivity towards linear disulfides.

Claims

exact text as granted — not AI-modified
The invention claimed is: 
     
       1. A process for the preparation of polysulfide of formula (I)
   HS—(CH 2 ) n —O—(CH 2 ) m —O—(CH 2 ) p —[S—S—(CH 2 ) n —O—(CH 2 ) m —O—(CH 2 ) p ] q —SH   (I)
 
 wherein m is an integer in the range 1 to 4, n and p are integers in the range 1-10, and q is an integer in the range 1-60, 
 by oxidizing a bismercaptodiether compound of formula (II)
   HS—(CH 2 ) n —O—(CH 2 ) m —O—(CH 2 ) p —SH   (II)
 
 
 with elemental sulfur in the presence of a base and a protic solvent. 
 
     
     
       2. The process according to  claim 1  wherein m=1. 
     
     
       3. The process according to  claim 1  wherein n=p=2. 
     
     
       4. The process according to  claim 1  wherein the protic solvent is an alcohol. 
     
     
       5. The process according to  claim 4  wherein the alcohol is methanol, ethanol or isopropanol. 
     
     
       6. The process according to  claim 1  wherein the base is a quaternary ammonium compound, a tertiary amine, or an inorganic base. 
     
     
       7. The process according to  claim 6  wherein the base is triethylamine or NaOH. 
     
     
       8. The process according to  claim 1  wherein the molar ratio elemental sulfur:bismercaptoether is in the range 0.5:1 to 1.2:1. 
     
     
       9. The process according to  claim 8  wherein the molar ratio elemental sulfur:bismercaptoether is in the range 0.7:1 to 0.99:1. 
     
     
       10. The process according to  claim 1  wherein the process is performed at a temperature in the range 60-85° C. 
     
     
       11. A process for the preparation of a liquid polysulfide of formula (I)
   HS—(CH 2 ) n —O—(CH 2 ) m —O—(CH 2 ) p —[S—S—(CH 2 ) n —O—(CH 2 ) m —O—(CH 2 ) p ] q —SH   (I)
 
 wherein m is an integer in the range 1 to 4, n and p are integers in the range 1-10, and q is an integer in the range 1-60, 
 by oxidizing a bismercaptodiether compound of formula (II)
   HS—(CH 2 ) n —O—(CH 2 ) m —O—(CH 2 ) p —SH   (II)
 
 
 with elemental sulfur in the presence of a base and a protic solvent.

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